CN108776149A - A method of titanium and titanium alloy ingot casting super large crystal grain is characterized by anode oxidation method - Google Patents
A method of titanium and titanium alloy ingot casting super large crystal grain is characterized by anode oxidation method Download PDFInfo
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- CN108776149A CN108776149A CN201810319824.3A CN201810319824A CN108776149A CN 108776149 A CN108776149 A CN 108776149A CN 201810319824 A CN201810319824 A CN 201810319824A CN 108776149 A CN108776149 A CN 108776149A
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- anodic oxidation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/2055—Analysing diffraction patterns
Abstract
The present invention provides a kind of method of characterization titanium or titanium alloy super large crystal grain, including：Anodic oxidation is carried out to titanium or titanium alloy sample, the sample surfaces after being dyed to anodic oxidation are taken pictures；Sample after oxidising dyeing has several color, and choosing at least two pieces from each color region is used as representative sample, carries out X-ray diffraction, obtains the crystalline phase of representative sample；The crystalline phase in other regions identical with representative sample color is identical as the crystalline phase of corresponding representative sample；If the diffraction the intensity of spectral line on a certain color region representative sample surface is smaller, diffraction can not be formed, then supplements and carries out pole figure experiment, measure the single phase property and orientation of the color region representative sample；The crystalline phase in other regions identical to representative sample color and the single phase property of corresponding representative sample and equally oriented.Present inventive concept is ingenious, while characterizing surface topography, the orientation of crystal grain is determined by x-ray diffraction experiment and pole figure experiment, can be widely used for the characterization of similar EB stove cast titanium ingot super large crystal grain as-cast structures.
Description
Technical field
The present invention relates to a kind of characterization grain morphology and the methods of orientation, especially with regard to a kind of EB stoves cast titanium ingot as cast condition
Organize the characterizing method of super large crystal grain.
Background technology
Titanium has that density is small, specific strength is high, thermal coefficient is low, high temperature resistant low temperature performance well, corrosion resistance are strong, one's own object
Property etc. prominent feature.Currently, as the use in fields such as the military projects such as aerospace, naval vessel, submarine, guided missile, high-tech is got over
Come more extensive, requirement is higher and higher, to for process the quality requirement of titanium and titanium alloy ingot casting also get up it is higher.Electron beam
Cold hearth (EBCHR) is the main method when former manufacture titanium or titanium alloy ingot, relative to traditional vacuum consumable smelting stove
(VAR), its advantage is that high density can be removed to be mingled with and be mingled with low-density, and can produce the square ingot, flat of different size
Ingot.The coarse grains of EB stove cast titanium ingots, there is certain orientation, are influenced on following process very big.Accurately characterize EB stove titanium ingots
Pattern and orientation be titanium ingot production and processing in an important topic.
Most important at present is to use Kroll reagent corrosion tables to EB stoves casting titanium or titanium alloy macroscopic view metallographic observation method
It is directly observed behind face, this method, and completely can not be true in the crystal boundary for telling different crystal grain that many times cannot be apparent
The orientation for determining crystal grain cannot provide enough data, such as according to the orientation rule of crystal grain group to short route processing such as direct cold rolling
Set the parameters such as rolling direction, rolling temperature.
Whether industrially pure titanium or low-alloy degree titanium alloy, the volume fraction of α phases all account for the overwhelming majority.The crystal of α phases
Structure belongs to hexagonal crystal system, and each main interplanar atomic density difference is apparent.The crystallite dimension of EB stove cast titanium ingots reaches li
Rice magnitude, complete characterization grain morphology, the sectional area of required sample is larger, generally reaches 50cm2More than.Meet 1A/cm2-
2A/cm2Current density, it is desirable to use high-power constant voltage dc source；The voltage of anodic oxidation is different, different crystal faces
Oxidation color can change, so needing to design a set of experimental method carrys out super large crystal grain carry out table to EB stove cast titanium ingots
Sign.
Invention content
The object of the present invention is to provide one kind to be easy to implement, effective experimental method characterizes titanium or titanium alloy super large
The pattern and orientation of crystal grain.
The method of characterization titanium or titanium alloy super large crystal grain provided by the present invention, includes the following steps：
1) anodic oxidation is carried out to titanium or titanium alloy sample to be characterized, after the completion of anodic oxidation, anodic oxidation is dyed
Sample surfaces afterwards are taken pictures；
2) sample after oxidising dyeing has several color, and choosing at least two pieces from each color region is used as representative sample
Product carry out X-ray diffraction, obtain the crystalline phase of representative sample；The crystalline phase in other regions identical to representative sample color with it is corresponding
The crystalline phase of representative sample is identical；
3) if the diffraction the intensity of spectral line on a certain color region representative sample surface is smaller, diffraction can not be formed, then is supplemented
Pole figure experiment is carried out, the single phase property and orientation of the color region representative sample are measured；Other areas identical with representative sample color
The single phase property of the crystalline phase in domain and corresponding representative sample and equally oriented.
In above method step 1), titanium or titanium alloy sample to be characterized is processed into the sheet sample of 5-10mm thickness first
Product, the sample are preferably rectangle sample, facilitate subsequent use clamping device to fix, and increase connecing between sample and clamping device
Contacting surface is accumulated, and local current is reduced.
The sheet sample first passes through polishing, etching operation before carrying out anodic oxidation experiment.
The concrete operations of the polishing are：Sheet sample is passed through to 120 mesh, 500 mesh, 1000 mesh, 2000 mesh respectively successively
Sand paper is polished.
The corrosion is：It is 5 by the sample volume ratio after polishing：10：85 HF：HNO3：H2O reagents are corroded
1min。
In the anodic oxidation experiment, the composition and ratio of used electrolyte are as follows：
The concrete operations of anodic oxidation experiment are：Sheet sample is fixed on clamping device, by power supply output line
Electrode line is connected to clamping device, and negative line is connected on cathode plate；The electrolyte prepared is put into electrolytic cell, cathode plate is put into
In electrolytic cell；Power supply is opened, setting electric current maximum value sets voltage value；Clamping device is held, together by clamping device and sample
It is put into progress anodic oxidation experiment in electrolyte.
In aforesaid operations, the depth of the electrolyte in a cell reaches 30mm or more.
The current maxima is according to formula I (A)=S (cm2) × 1.5 are calculated, wherein S is the sectional area of sample.
The voltage value is set as 20V.
Sample face to be oxidized is maintained at 20mm or so, anodizing time with the cathode distance between plates in anodic oxidation experiment
Can be 10s-20s.
Further include by sample from folder before sample surfaces after being dyed to anodic oxidation after the completion of anodic oxidation are taken pictures
It holds and is unclamped on tool, the operation of the sample surfaces after cleaning dyeing.
Further include the behaviour cleaned to dyeing face using Kroll reagents before carrying out x-ray diffraction experiment to sample
Make.
The present invention has the following advantages due to taking above technical scheme：1, purposes of the invention is that characterization titanium and titanium close
The pattern and orientation of golden super large crystal grain, experiment is easy to implement, applied widely；According to the area of laboratory sample, selection is suitable
Current Voltage carries out anodic oxidation experiment to large scale piece sample.2, anodic oxidation experiment is carried out to titanium and titanium using suitable voltage
Alloy carries out colour metallograpy characterization, and used voltage is bigger, and the oxidation film that is formed is thicker after anodic oxidation experiment, and color is also
It is deeper；When voltage is 20V, the discrimination degree of obtained colour metallograpy is best.3, this experimental method can be used for characterizing grain shaped
While looks, the orientation of crystal grain can also be determined；Since cooling rate is different everywhere for titanium slab ingot, there are a degree of for crystal grain
Preferred orientation, after carrying out anodic oxidation experiment using 20V voltages, basal plane is in golden yellow, and other crystal faces are according to the angle with basal plane
Purple is gradually become by golden yellow.
Present inventive concept is ingenious, the titanium or titanium alloy sample of super large crystal grain and anodic oxidation experiment is combined, in table
While levying surface topography, the orientation of crystal grain is can determine by x-ray diffraction experiment and pole figure experiment, can be widely used for similar EB
The characterization of stove cast titanium ingot super large crystal grain as-cast structure.
Description of the drawings
Fig. 1 is anodic oxidation experimental method schematic diagram of the present invention.In Fig. 1,1 is cathode plate；2 be clamping device；3 be electrolysis
Slot；4 be electrolyte；5 be sample, and cathode plate and clamping device are stainless steel material.
Fig. 2 is the metallograph obtained after anodic oxidation is tested.
Fig. 3 is the XRD Determination of Orientation result and pole figure experimental result of the identical crystal grain of anodic oxidation color.(a) is in Fig. 3
The oxidation color of 1# crystal grain；(b) it is the XRD spectrums of 1# crystal grain；(c) it is the oxidation color of 2# crystal grain；(d) it is 2# crystal grain
XRD spectrums；(e) it is the pole figure experimental result of 2# crystal grain.
Anodic oxidation experimental result comparison when Fig. 4 is using 20V and 30V voltages.
Specific implementation mode
Below by specific embodiment, the present invention will be described, but the present invention is not limited thereto.
Experimental method used in following embodiments is conventional method unless otherwise specified；Institute in following embodiments
Reagent, material etc., are commercially available unless otherwise specified.
Embodiment
One, sample anodes aoxidize
1, sample is processed into the sheet sample 5 of 5mm thickness, preferably rectangle sample first, clamping device is facilitated to fix sample,
And the contact area between sample and clamping device 2 is increased, reduce local current.
2, sheet sample 5 is 5 with volume ratio respectively after 120 mesh, 500 mesh, 1000 mesh, the polishing of 2000 mesh sand paper：
10：85 HF：HNO3：H2O reagents carry out corrosion 1min.
3, in the present embodiment to electrolyte 4 without temperature requirement, can be tested in room temperature.The proportioning of electrolyte 4 is as follows：
4, sheet sample 5 is fixed on clamping device 2, power supply output line electrode line is connected to clamping device 2, negative line
It is connected on cathode plate 1.
5, the electrolyte 4 prepared is put into electrolytic cell 3, cathode plate is put into electrolytic cell 3, it is ensured that the depth of electrolyte
Reach 30mm or more.
6, power supply is opened, according to sample area setting electric current maximum value, I (A)=S (cm2) × 1.5, S is sample in cross section
Product, voltage are set as 20V.
7, clamping device 2 is held, clamping device 2 and sample 5 are put into togerther progress anodic oxidation experiment in electrolyte 4,
Distance is maintained at 20mm or so, anodizing time 10s-20s between sample 5 and cathode plate 1.
8, sample 5 is unclamped from clamping device 2 after the completion of anodic oxidation, to the sample surfaces after anodic oxidation after cleaning
It takes pictures.
The metallograph obtained after anodic oxidation experiment is as shown in Figure 2.
Two, crystal grain verification and Determination of Orientation
1, the region that same color is chosen from the sample after oxidising dyeing, is processed into blocky X-ray diffraction sample, sample
Quantity is several, two samples of at least making of same color.
2, after face cleaning will be dyed using Kroll reagents, x-ray diffraction experiment is carried out, determines that color same area only has
One crystalline phase.
3, the diffraction the intensity of spectral line on such as fruit block sample surface is smaller, is that can not form diffraction since crystal face is parallel with X-ray,
Pole figure experiment is then supplemented, to measure the single phase property and orientation of crystal grain.
Fig. 3 is the XRD Determination of Orientation result and pole figure experimental result of the identical crystal grain of anodic oxidation color.(a) is in Fig. 3
The oxidation color of 1# crystal grain；(b) it is the XRD spectrums of 1# crystal grain；(c) it is the oxidation color of 2# crystal grain；(d) it is 2# crystal grain
XRD spectrums；(e) it is the pole figure experimental result of 2# crystal grain.
4, the single phase property of crystal grain is determined by the X-ray diffraction and pole figure experimental result that compare same color region and taken
To.
Three, relationship of the atomic density of the crystal face of hexagonal crystal system to when titanium oxide layer thickness and color
1, the parameter of typical crystal face see the table below in hexagonal crystal system：
| Crystal face | Crystal face atomic density | Interplanar distance |
| Bottom surface (0 00 1) | 0.385/a2 | 1.633a |
| Prismatic surface (1 0-1 0) | 0.408/a2 | 0.865a |
| Pyramidal surface (- 101 1) | 0.791/a2 | 0.585a |
2, the relationship of oxidated layer thickness and anodic oxidation experiment parameter
Can explain the formation of titanium surface color and polish with two theories under normal conditions, when oxide on surface chemistry at
It is point different to cause observed surface color different；Second is that due to caused by interplanar optical interference.Ni―Ti anode oxygen
Surface color and polish after change belong to the interference of light as a result, and there is no surface formed pigment.So influencing the anodic oxidation face of titanium
The leading factor of color is optical interference, and the principal element for influencing optical interference is oxidated layer thickness.The calculating of oxidated layer thickness
It can be obtained by following formula：
Wherein, d is the thickness of oxide layer, unit nm, λmaxIt is the maximum absorption wavelength of oxide layer, unit nm, n0It is
Refraction coefficient.Refraction coefficient in titanium oxide layer is different with maximum absorption wavelength difference, can be calculated by following formula：
The scope of application that above formula calculates oxidated layer thickness is d>20nm will produce oxygen if oxidated layer thickness is too small
The synergistic effect for changing layer island growth, influences color judgement, and when 20nm, corresponding anodic oxidation voltage was 2V.The above coefficient n0
The tissue smaller suitable for crystallite dimension, to the larger tissue of crystallite dimension, each interplanar refraction coefficient has difference, so being formed
Oxidated layer thickness it is inconsistent, different surface face will be showed on different crystal grain under same anodic oxidation condition
Color.
3, the correspondence of titanium oxide layer thickness and color
Comparative example
With reference to the method in embodiment, it sets anodic oxidation voltage to 30V, other parameter constant, after anodic oxidation
Sample surfaces take pictures.Its metallograph is as shown in Figure 4.
As shown in Figure 4：As shown in Figure 4, when the voltage of selection is 30V, whole anodic oxidation color is light blue, discrimination
Degree is not high, not as good as yellow purple region discrimination degree is high when using voltage as 20V.
Claims (9)
1. a kind of method of characterization titanium or titanium alloy super large crystal grain, includes the following steps：
1) anodic oxidation is carried out to titanium or titanium alloy sample to be characterized, after the completion of anodic oxidation, after being dyed to anodic oxidation
Sample surfaces are taken pictures；
2) sample after oxidising dyeing has several color, and choosing at least two pieces from each color region is used as representative sample, into
Row X-ray diffraction obtains the crystalline phase of representative sample；The crystalline phase in other regions identical to representative sample color and corresponding representative sample
The crystalline phase of product is identical；
3) if the diffraction the intensity of spectral line on a certain color region representative sample surface is smaller, diffraction can not be formed, then supplements progress
Pole figure is tested, and the single phase property and orientation of the color region representative sample are measured；Other regions identical with representative sample color
The single phase property of crystalline phase and corresponding representative sample and equally oriented.
2. according to the method described in claim 1, it is characterized in that：In step 1), first by titanium or titanium alloy sample to be characterized
Product are processed into the sheet sample of 5-10mm thickness；
The sheet sample first passes through polishing, etching operation before carrying out anodic oxidation.
3. according to the method described in claim 2, it is characterized in that：The operation of the polishing is：Sheet sample is distinguished successively
By 120 mesh, 500 mesh, 1000 mesh, the polishing of 2000 mesh sand paper；
The corrosion is：It is 5 by the sample volume ratio after polishing：10：85 HF：HNO3：H2O reagents carry out corrosion 1min.
4. method according to any one of claim 1-3, it is characterised in that：In step 1), in the anodic oxidation, institute
The composition and ratio of the electrolyte of use are as follows：
Oxalic acid 75g；Citric acid 75g；Phosphoric acid 75ml；Alcohol 900ml；Lactic acid 1500ml；Water 525ml.
5. according to the described method of any one of claim 1-4, it is characterised in that：In step 1), the anodic oxidation experiment
Operation be：Sheet sample is fixed on clamping device, power supply output line electrode line is connected to clamping device, negative line is connected to
On cathode plate；Electrolyte is put into electrolytic cell, cathode plate is put into electrolytic cell；Opening power supply, setting electric current maximum value, if
Constant voltage value；Clamping device is held, clamping device and sample are put into togerther progress anodic oxidation experiment in electrolyte.
6. according to the method described in claim 5, it is characterized in that：The depth of the electrolyte in a cell reach 30mm with
On；
The current maxima is according to formula I (A)=S (cm2) × 1.5 are calculated, wherein S is the sectional area of sample；
Sample face to be oxidized is maintained at 18-22mm with the cathode distance between plates in anodic oxidation experiment, and anodizing time is
10s-20s。
7. according to the method described in any one of claim 1-6, it is characterised in that：The voltage value is set as 20V.
8. according to the described method of any one of claim 1-7, it is characterised in that：Anodic oxidation is contaminated after the completion of anodic oxidation
Further include unclamping sample from clamping device before sample surfaces after color are taken pictures, the sample surfaces after cleaning dyeing
Operation.
9. according to the method described in any one of claim 1-8, it is characterised in that：X-ray diffraction experiment is being carried out to sample
Before, further include the operation cleaned to dyeing face using Kroll reagents.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810319824.3A CN108776149B (en) | 2018-04-11 | 2018-04-11 | Method for representing oversized grains of titanium and titanium alloy ingots by anodic oxidation method |
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| CN201810319824.3A CN108776149B (en) | 2018-04-11 | 2018-04-11 | Method for representing oversized grains of titanium and titanium alloy ingots by anodic oxidation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110455793A (en) * | 2019-08-29 | 2019-11-15 | 佛山市安齿生物科技有限公司 | Method for distinguishing pure titanium and titanium alloy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110455793A (en) * | 2019-08-29 | 2019-11-15 | 佛山市安齿生物科技有限公司 | Method for distinguishing pure titanium and titanium alloy |
| CN110455793B (en) * | 2019-08-29 | 2021-12-14 | 佛山市安齿生物科技有限公司 | Method for distinguishing pure titanium and titanium alloy |
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